CN114369493A - Preparation method of biodegradable water-resistant shield tail sealing grease - Google Patents

Preparation method of biodegradable water-resistant shield tail sealing grease Download PDF

Info

Publication number
CN114369493A
CN114369493A CN202011101714.3A CN202011101714A CN114369493A CN 114369493 A CN114369493 A CN 114369493A CN 202011101714 A CN202011101714 A CN 202011101714A CN 114369493 A CN114369493 A CN 114369493A
Authority
CN
China
Prior art keywords
grease
particle size
preparation
stirring
solid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011101714.3A
Other languages
Chinese (zh)
Inventor
王树贞
马磊
于洋洋
宗磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Qingyishan Petrochemical Technology Co ltd
Original Assignee
Shandong Qingyishan Petrochemical Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shandong Qingyishan Petrochemical Technology Co ltd filed Critical Shandong Qingyishan Petrochemical Technology Co ltd
Priority to CN202011101714.3A priority Critical patent/CN114369493A/en
Publication of CN114369493A publication Critical patent/CN114369493A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06Mixtures of thickeners and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M121/00Lubricating compositions characterised by the thickener being a compound of unknown or incompletely defined constitution
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/102Silicates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/023Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/046Overbasedsulfonic acid salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066Thiocarbamic type compounds
    • C10M2219/068Thiocarbamate metal salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/04Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions having a silicon-to-carbon bond, e.g. organo-silanes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/045Siloxanes with specific structure containing silicon-to-hydroxyl bonds

Abstract

The invention relates to the technical field of sealing grease, in particular to a preparation method of biodegradable water-resistant shield tail sealing grease. The preparation method comprises the steps of preparing a radish seed extract, preparing a buckeye extract, adding the radish seed extract, the buckeye extract, an antioxidant, an antirust agent, an oiliness agent, a structure stabilizer and a multi-effect additive into basic fat, uniformly stirring, and sequentially adding the solid additive in batches according to the particle size. According to the lubricating grease, the radish seeds contain erucic acid, linoleic acid, linolenic acid and erucic acid glyceride in the amount after being extracted by the extraction process, so that the degradation effect of base oil can be effectively improved, the addition of the buckeye seed extract can play a role in thickening and improve the waterproof effect of the lubricating grease, and solid additives with different particle size distributions are added into the lubricating grease, so that the sealing property and the water resistance of the lubricating grease are enhanced.

Description

Preparation method of biodegradable water-resistant shield tail sealing grease
Technical Field
The invention relates to the technical field of sealing grease, in particular to a preparation method of biodegradable water-resistant shield tail sealing grease.
Background
The shield tunneling machine is a preferred excavating tool for excavating urban subway tunnels, has the advantages of no influence of ground buildings and geographic environments, is particularly wide in application range, and can completely meet the strict requirements of urban tunnel construction. The shield tail sealing system is a sealing device designed for preventing soil layers, sand layers, water layers and slurry around the shield tail from entering the shield machine from gaps between the shield tail and the duct piece. The shield tail sealing grease is injected into a sealing cavity between three rows of stainless steel wire brushes from the shield tail through a grease pump in real time and keeps a dynamic full state so as to meet the requirements of sealing and protecting shield construction. Generally, shield tail grease consumption of a shield machine (diameter is 6.4 m) for urban subways is about 20-40 kg/m, special stratum consumption is 80-100 kg/m, and shield tail grease consumption per kilometer is 20-40 tons on average.
The blocking capability and biodegradability of the shield tail sealing grease to water and other liquids are important measurement indexes of the performance of the shield tail sealing grease, and technical personnel make a great deal of breakthrough researches aiming at the waterproofness and biodegradability of the shield tail sealing grease, such as: the Chinese patent application CN111394160A discloses a high-performance shield tail sealing grease which comprises the following components in parts by weight: 20-30 parts of vegetable oil, 15-23 parts of ethylene propylene rubber, 3-6 parts of reinforcing fiber, 0.5-1.5 parts of dispersing agent, 1-2 parts of bentonite, 5-10 parts of light calcium carbonate, 2-5 parts of boron nitride nanosheet/montmorillonite intercalated composite material and 1-5 parts of hollow mesoporous titanium dioxide. The shield tail sealing grease prepared by the technology has good water resistance and high temperature resistance, excellent sealing performance and good pumping performance, but the biodegradation rate of the shield tail sealing grease prepared by the technology is always lower than 95%.
Disclosure of Invention
The invention aims to provide a preparation method of biodegradable water-resistant shield tail sealing grease, which overcomes the defects of the prior art, and is characterized in that radish seed extract and buckeye seed extract are added into base grease forming lubricating grease to improve the water resistance and the biodegradability of the lubricating grease, and solid additives with different granularities are added into lubricating grease to ensure that the solid additives are uniformly dispersed in the lubricating grease like thickening agents, so that the water resistance and the sealing performance of the lubricating grease are enhanced.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a biodegradable water-resistant shield tail sealing grease is mainly composed of the following raw materials in parts by weight: 100-150 parts of lubricating grease, 5-45 parts of solid additive, 1-5 parts of antioxidant, 2-8 parts of antirust agent, 0.5-2 parts of oiliness agent, 2-5 parts of structure stabilizer and 1-3 parts of multi-effect additive.
Preferably, the material mainly comprises the following raw materials in parts by weight: 125 parts of lubricating grease, 28 parts of solid additive, 3 parts of antioxidant, 6 parts of antirust agent, 1.75 parts of oiliness agent, 4 parts of structure stabilizer and 2 parts of multi-effect additive.
Preferably, the lubricating grease mainly comprises base grease, radish seed extract and buckeye seed extract according to the weight ratio of (5-7): (3-2): (1-2), wherein the base grease is one or more of calcium grease, composite calcium grease, sodium grease, lithium grease, composite lithium grease, aluminum grease, composite aluminum grease, titanium grease, composite titanium grease, polyurea grease and composite polyurea grease.
Preferably, the solid additive is one or more of asbestos powder, calcium carbonate, plant fiber and composite fiber.
Preferably, the solid additive has a particle size ranging from 0.5 to 50 μm.
Preferably, the solid additives with the particle size of 0.5-10 μm in the solid additives account for 5-25% of the total weight of the solid additives, the solid additives with the particle size of 10-20 μm account for 20-50% of the total weight of the solid additives, the solid additives with the particle size of 20-40 μm account for 10-40% of the total weight of the solid additives, and the solid additives with the particle size of 40-50 μm account for 10-40% of the total weight of the solid additives.
Preferably, the antioxidant is prepared from 2, 6-di-tert-butyl-p-cresol, an alkylated group-alpha-naphthylamine and rosemary in a weight ratio of (1-3): 5: 1 is prepared by compounding.
Preferably, the antirust agent adopts one or a mixture of two of medium-base-number synthetic calcium sulfonate (T105) and high-base-number synthetic calcium sulfonate (T106).
Preferably, the oily agent is a long-chain organic acid type oily agent.
Preferably, the structure stabilizer is one or more of diphenyl dihydroxy silane, hydroxy silicone oil and hexamethyl disilazane, and the multi-effect additive is dialkyl dithiocarbamate.
A preparation method of biodegradable water-resistant shield tail sealing grease comprises the following preparation steps:
(1) preparing a radish seed extract: putting dried radish seed powder with the particle size of 150-; concentrating the filtrate, removing ethanol in the extract, and centrifuging to obtain concentrated solution; passing the centrifuged concentrated solution through chromatographic column, eluting with 2-6 times of 10-20 wt% ethanol or water, eluting with 2-6 times of 30-50 wt% ethanol, and collecting the eluate; concentrating the obtained eluate, removing ethanol from the concentrated solution, centrifuging the obtained concentrated solution, and drying with vacuum freeze dryer;
(2) preparing an buckeye seed extract: crushing buckeye seeds, sieving, performing ultrasonic extraction for 80-90min by using ethanol with the volume fraction of 85-95% according to the material-liquid ratio of 1:15-1:20, and concentrating the extracting solution to obtain an extract;
(3) weighing basic grease, adding radish seed extract, buckeye seed extract, antioxidant, antirust agent, oiliness agent, structure stabilizer and multi-effect additive, stirring at the speed of 180-;
(4) adding a solid additive with the particle size of 40-50 mu m into the lubricating paste mixture, stirring while adding at the stirring speed of 120-150r/min, stirring for 20-40min, then adding the solid additive with the particle size of 20-40 mu m, stirring while adding at the stirring speed of 80-120r/min, stirring for 30-40min, then adding the solid additive with the particle size of 10-20 mu m, stirring while adding at the stirring speed of 60-80r/min, stirring for 30-40min, then adding the solid additive with the particle size of 0.5-10 mu m, stirring while adding at the stirring speed of 40-60r/min, and stirring for 40-50 min.
The invention has the beneficial effects that: compared with the prior art, the preparation method of the biodegradable water-resistant shield tail sealing grease has the following advantages: (1) according to the lubricating grease disclosed by the invention, the radish seed extract and the buckeye extract are taken as main materials, the conventional basic grease is taken as an auxiliary material, the radish seed is extracted by the extraction process disclosed by the invention, and the erucic acid, linoleic acid, linolenic acid and erucic acid glyceride contained in the radish seed extract can effectively improve the degradation effect of the basic oil, and the addition of the buckeye extract can play a role in thickening and improve the waterproof effect of the lubricating grease; (2) the solid additives with different particle size distributions are added into the lubricating grease, and the solid additives are adhered to the radish seed extract and the semen aesculi extract, so that the solid additives are uniformly dispersed among the basic grease like thickening agents, and the sealing property and the water resistance of the lubricating grease are enhanced.
Detailed Description
Example 1
A biodegradable water-resistant shield tail sealing grease is mainly composed of the following raw materials in parts by weight: 125 parts of lubricating grease, 28 parts of solid additive, 3 parts of antioxidant, 6 parts of antirust agent, 1.75 parts of oiliness agent, 4 parts of structure stabilizer and 2 parts of multi-effect additive.
The lubricating grease is prepared from basic grease, a radish seed extract and a buckeye extract according to the weight ratio of 6: 2: 1, wherein the basic grease is composite aluminum-based grease; the solid additive is asbestos powder and plant fiber; the particle size range of the solid additive is 0.5-50 μm, wherein the solid additive with the particle size of 0.5-10 μm accounts for 15% of the total weight of the solid additive, the solid additive with the particle size of 10-20 μm accounts for 35% of the total weight of the solid additive, the solid additive with the particle size of 20-40 μm accounts for 25% of the total weight of the solid additive, and the solid additive with the particle size of 40-50 μm accounts for 25% of the total weight of the solid additive.
The antioxidant is prepared from 2, 6-di-tert-butyl-p-cresol, alkylated-alpha-naphthylamine and rosemary according to the weight ratio of 2: 5: 1 is prepared by compounding. The rust inhibitor adopts medium-base-number synthetic calcium sulfonate (T105). The oiliness agent is a long-chain organic acid oiliness agent. The structure stabilizer adopts diphenyl dihydroxy silane. The multi-effect additive is a dialkyl dithiocarbamate.
A preparation method of biodegradable water-resistant shield tail sealing grease comprises the following preparation steps:
(1) preparing a radish seed extract: putting dried radish seed powder with the particle size of 200 mu m and 85 wt% of ethanol solution into a cavity of ultrasonic-microwave synergistic extraction equipment for extraction, wherein the mass of the ethanol solution is 7 times of that of the radish seed powder, extracting for 3 times, cooling after extraction is finished, filtering the extracting solution by using a 180-mesh screen to obtain filtrate, and combining the filtrate; concentrating the filtrate, removing ethanol in the extract, and centrifuging to obtain concentrated solution; passing the centrifuged concentrated solution through a chromatographic column, eluting with 4 times of column volume of 15 wt% ethanol or water to remove impurities, eluting with 4 times of column volume of 40 wt% ethanol, and collecting the eluate; concentrating the obtained eluate, removing ethanol from the concentrated solution, centrifuging the obtained concentrated solution, and drying with vacuum freeze dryer;
(2) preparing an buckeye seed extract: crushing and sieving Chinese buckeye seeds, ultrasonically extracting for 85min by using 90% ethanol according to a material-liquid ratio of 1:18, and concentrating an extracting solution to obtain an extract;
(3) weighing basic grease, adding radish seed extract, semen Aesculi extract, antioxidant, antirust agent, oiliness agent, structure stabilizer and multi-effect additive, stirring at 220r/min for 30min to obtain lubricating grease mixture;
(4) adding solid additive with the particle size of 40-50 mu m into the lubricating paste mixture, stirring while adding at the stirring speed of 135r/min, stirring for 30min, then adding solid additive with the particle size of 20-40 mu m, stirring while adding at the stirring speed of 100r/min, stirring for 35min, then adding solid additive with the particle size of 10-20 mu m, stirring while adding at the stirring speed of 70r/min, stirring for 35min, then adding solid additive with the particle size of 0.5-10 mu m, stirring while adding at the stirring speed of 50r/min, and stirring for 45 min.
Example 2
A biodegradable water-resistant shield tail sealing grease is mainly composed of the following raw materials in parts by weight: 100 parts of lubricating grease, 10 parts of solid additive, 2 parts of antioxidant, 2 parts of antirust agent, 0.5 part of oiliness agent, 2 parts of structure stabilizer and 1 part of multi-effect additive.
The lubricating grease is prepared from basic grease, a radish seed extract and a buckeye extract according to a weight ratio of 5: 3: 1, wherein the basic grease is a composite titanium grease. The solid additive is formed by doping asbestos powder, calcium carbonate and composite fibers. The particle size range of the solid additive is 0.5-50 μm. In the solid additives, the solid additives with the particle size of 0.5-10 mu m account for 10 percent of the total weight of the solid additives, the solid additives with the particle size of 10-20 mu m account for 20 percent of the total weight of the solid additives, the solid additives with the particle size of 20-40 mu m account for 30 percent of the total weight of the solid additives, and the solid additives with the particle size of 40-50 mu m account for 40 percent of the total weight of the solid additives.
The antioxidant is prepared from 2, 6-di-tert-butyl-p-cresol, alkylated-alpha-naphthylamine and rosemary according to the weight ratio of 1: 5: 1 is prepared by compounding. The antirust agent adopts high-base-number synthetic calcium sulfonate (T106). The oiliness agent is a long-chain organic acid oiliness agent. The structure stabilizer adopts hexamethyldisilazane, and the multi-effect additive is dialkyl dithiocarbamate.
A preparation method of biodegradable water-resistant shield tail sealing grease comprises the following preparation steps:
(1) preparing a radish seed extract: putting dried radish seed powder with the particle size of 150 mu m and 80 wt% of ethanol solution into a cavity of ultrasonic-microwave synergistic extraction equipment for extraction, wherein the mass of the ethanol solution is 6 times of that of the radish seed powder, extracting for 2 times, cooling after extraction is finished, filtering the extracting solution by using a 150-mesh screen to obtain filtrate, and combining the filtrate; concentrating the filtrate, removing ethanol in the extract, and centrifuging to obtain concentrated solution; passing the centrifuged concentrated solution through a chromatographic column, eluting impurities with 2 times of 10 wt% ethanol or water, eluting with 2 times of 30 wt% ethanol, and collecting the eluate; concentrating the obtained eluate, removing ethanol from the concentrated solution, centrifuging the obtained concentrated solution, and drying with vacuum freeze dryer;
(2) preparing an buckeye seed extract: crushing buckeye seeds, sieving, ultrasonically extracting for 80min by using ethanol with the volume fraction of 85% according to the material-liquid ratio of 1:15, and concentrating the extracting solution to obtain an extract;
(3) weighing basic grease, adding radish seed extract, semen Aesculi extract, antioxidant, antirust agent, oiliness agent, structure stabilizer and multi-effect additive, stirring at 180r/min for 20min to obtain lubricating grease mixture;
(4) adding solid additive with the particle size of 40-50 mu m into the lubricating paste mixture, stirring while adding at the stirring speed of 120r/min for 20min, then adding solid additive with the particle size of 20-40 mu m, stirring while adding at the stirring speed of 80r/min for 30min, then adding solid additive with the particle size of 10-20 mu m, stirring while adding at the stirring speed of 60r/min for 30min, then adding solid additive with the particle size of 0.5-10 mu m, stirring while adding at the stirring speed of 40r/min, and stirring for 40 min.
Example 3
A biodegradable water-resistant shield tail sealing grease is mainly composed of the following raw materials in parts by weight: 150 parts of lubricating grease, 45 parts of solid additive, 5 parts of antioxidant, 8 parts of antirust agent, 2 parts of oiliness agent, 5 parts of structure stabilizer and 3 parts of multi-effect additive.
The lubricating grease is prepared from basic grease, a radish seed extract and a buckeye extract according to a weight ratio of 7: 2: 2, wherein the basic grease is formed by mixing calcium-based grease and sodium-based grease. The solid additive is formed by mixing calcium carbonate and plant fiber. The particle size range of the solid additive is 0.5-50 μm. In the solid additives, the solid additives with the particle size of 0.5-10 mu m account for 20 percent of the total weight of the solid additives, the solid additives with the particle size of 10-20 mu m account for 40 percent of the total weight of the solid additives, the solid additives with the particle size of 20-40 mu m account for 20 percent of the total weight of the solid additives, and the solid additives with the particle size of 40-50 mu m account for 20 percent of the total weight of the solid additives.
The antioxidant is prepared from 2, 6-di-tert-butyl-p-cresol, alkylated-alpha-naphthylamine and rosemary according to the weight ratio of 3: 5: 1 is prepared by compounding. The antirust agent adopts high-base-number synthetic calcium sulfonate (T106). The oiliness agent is a long-chain organic acid oiliness agent. The structure stabilizer adopts hydroxyl silicone oil, and the multi-effect additive is dialkyl dithiocarbamate.
A preparation method of biodegradable water-resistant shield tail sealing grease comprises the following preparation steps:
(1) preparing a radish seed extract: putting dried radish seed powder with the particle size of 300 mu m and 95 wt% of ethanol solution into a cavity of ultrasonic-microwave synergistic extraction equipment for extraction, wherein the mass of the ethanol solution is 8 times of that of the radish seed powder, extracting for 4 times, cooling after extraction is finished, filtering the extracting solution by using a 200-mesh screen to obtain filtrate, and combining the filtrate; concentrating the filtrate, removing ethanol in the extract, and centrifuging to obtain concentrated solution; passing the centrifuged concentrated solution through a chromatographic column, eluting impurities with 6 times of column volume of 20 wt% ethanol or water, eluting with 6 times of column volume of 50 wt% ethanol, and collecting the eluate; concentrating the obtained eluate, removing ethanol from the concentrated solution, centrifuging the obtained concentrated solution, and drying with vacuum freeze dryer;
(2) preparing an buckeye seed extract: crushing buckeye seeds, sieving, ultrasonically extracting for 90min by using 95% ethanol according to a material-liquid ratio of 1:20, and concentrating an extracting solution to obtain an extract;
(3) weighing basic grease, adding radish seed extract, semen Aesculi extract, antioxidant, antirust agent, oiliness agent, structure stabilizer and multi-effect additive, stirring at 260r/min for 40min to obtain lubricating grease mixture;
(4) adding solid additive with the particle size of 40-50 mu m into the lubricating paste mixture, stirring while adding at the stirring speed of 150r/min for 40min, then adding solid additive with the particle size of 20-40 mu m, stirring while adding at the stirring speed of 120r/min for 40min, then adding solid additive with the particle size of 10-20 mu m, stirring while adding at the stirring speed of 80r/min for 40min, then adding solid additive with the particle size of 0.5-10 mu m, stirring while adding at the stirring speed of 60r/min, and stirring for 50 min.
Comparative example 1
Comparative example 1 is essentially the same as example 1 except that: the lubricating grease mainly comprises basic grease, radish seed extract and buckeye extract according to the weight ratio of 8: 2: 1.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that: in the solid additives described in comparative example 2, the solid additives having a particle size of 0.5 to 10 μm were 30% by weight, the solid additives having a particle size of 10 to 20 μm were 10% by weight, the solid additives having a particle size of 20 to 40 μm were 30% by weight, and the solid additives having a particle size of 40 to 50 μm were 30% by weight, based on the total weight of the solid additives.
Test example 1
The biodegradable water-resistant tail sealing greases prepared in examples 1 to 3, comparative example 1 and comparative example 2 were subjected to performance tests, and the test results are shown in table 1:
TABLE 1
Figure BDA0002725585240000081
As can be seen from Table 1, the lubricating grease disclosed by the invention effectively improves the degradation effect of the base oil by adding the radish seed extract and the buckeye extract in a reasonable proportion, and the biodegradation rate is as high as 98.9%. According to the invention, solid additives with different particle size distributions are added into the lubricating grease according to a reasonable proportion, and the solid additives are adhered to the radish seed extract and the semen aesculi extract, so that the solid additives are uniformly dispersed among the basic grease like a thickening agent, and the sealing property and the water resistance of the lubricating grease are enhanced.
The above embodiments are only specific examples of the present invention, and the protection scope of the present invention includes but is not limited to the product forms and styles of the above embodiments, and any suitable changes or modifications made by those skilled in the art according to the claims of the present invention shall fall within the protection scope of the present invention.

Claims (5)

1. A preparation method of biodegradable water-resistant shield tail sealing grease is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
s1, weighing 150 parts of lubricating grease 100, 5-45 parts of solid additive, 1-5 parts of antioxidant, 2-8 parts of antirust agent, 0.5-2 parts of oiliness agent, 2-5 parts of structure stabilizer and 1-3 parts of multi-effect additive, wherein the lubricating grease mainly comprises base grease, radish seed extract and buckeye seed extract according to the weight ratio (5-7): (3-2): (1-2);
s2, adding a radish seed extract, a semen aesculi extract, an antioxidant, an antirust agent, an oiliness agent, a structure stabilizer and a multi-effect additive into the base grease, stirring at the speed of 180-260r/min for 20-40min to obtain a lubricating grease mixture;
s3, adding a solid additive with the particle size of 40-50 mu m into the lubricating paste mixture, stirring while adding at the stirring speed of 120-150r/min, stirring for 20-40min, then adding the solid additive with the particle size of 20-40 mu m, stirring while adding at the stirring speed of 80-120r/min, stirring for 30-40min, then adding the solid additive with the particle size of 10-20 mu m, stirring while adding at the stirring speed of 60-80r/min, stirring for 30-40min, then adding the solid additive with the particle size of 0.5-10 mu m, stirring while adding at the stirring speed of 40-60r/min, and stirring for 40-50 min.
2. The preparation method of the biodegradable water-resistant shield tail sealing grease as claimed in claim 1, wherein the preparation method comprises the following steps: the preparation method of the radish seed extract comprises the following steps: putting dried radish seed powder with the particle size of 150-; concentrating the filtrate, removing ethanol in the extract, and centrifuging to obtain concentrated solution; passing the centrifuged concentrated solution through chromatographic column, eluting with 2-6 times of 10-20 wt% ethanol or water, eluting with 2-6 times of 30-50 wt% ethanol, and collecting the eluate; concentrating the obtained eluate, removing ethanol from the concentrated solution, centrifuging the obtained concentrated solution, and drying with vacuum freeze dryer.
3. The preparation method of the biodegradable water-resistant shield tail sealing grease as claimed in claim 1, wherein the preparation method comprises the following steps: the preparation method of the buckeye seed extract comprises the following steps: crushing buckeye seeds, sieving, performing ultrasonic extraction for 80-90min by using ethanol with the volume fraction of 85-95% according to the material-liquid ratio of 1:15-1:20, and concentrating the extracting solution to obtain an extract.
4. The preparation method of the biodegradable water-resistant shield tail sealing grease as claimed in claim 1, wherein the preparation method comprises the following steps: the basic grease is one or more of calcium grease, composite calcium grease, sodium grease, lithium grease, composite lithium grease, aluminum grease, composite aluminum grease, titanium grease, composite titanium grease, polyurea grease and composite polyurea grease.
5. The preparation method of the biodegradable water-resistant shield tail sealing grease as claimed in claim 1, wherein the preparation method comprises the following steps: the solid additive is one or more of asbestos powder, calcium carbonate, plant fiber and composite fiber; the particle size range of the solid additive is 0.5-50 mu m; in the solid additives, the solid additives with the particle size of 0.5-10 mu m account for 5-25% of the total weight of the solid additives, the solid additives with the particle size of 10-20 mu m account for 20-50% of the total weight of the solid additives, the solid additives with the particle size of 20-40 mu m account for 10-40% of the total weight of the solid additives, and the solid additives with the particle size of 40-50 mu m account for 10-40% of the total weight of the solid additives.
CN202011101714.3A 2020-10-15 2020-10-15 Preparation method of biodegradable water-resistant shield tail sealing grease Pending CN114369493A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011101714.3A CN114369493A (en) 2020-10-15 2020-10-15 Preparation method of biodegradable water-resistant shield tail sealing grease

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011101714.3A CN114369493A (en) 2020-10-15 2020-10-15 Preparation method of biodegradable water-resistant shield tail sealing grease

Publications (1)

Publication Number Publication Date
CN114369493A true CN114369493A (en) 2022-04-19

Family

ID=81138025

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011101714.3A Pending CN114369493A (en) 2020-10-15 2020-10-15 Preparation method of biodegradable water-resistant shield tail sealing grease

Country Status (1)

Country Link
CN (1) CN114369493A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04337388A (en) * 1991-05-15 1992-11-25 Miyoshi Oil & Fat Co Ltd Metal working oil
CN1219842A (en) * 1996-04-26 1999-06-16 纳幕尔杜邦公司 Soybean oil having high oxidative stability
CN101153236A (en) * 2006-09-29 2008-04-02 中国石油化工股份有限公司 Water-resistant oleosol and method of producing the same
US20110033413A1 (en) * 2007-12-24 2011-02-10 Klaus Kwetkat Method for producing oil-in-water emulsions from self-emulsifying gel concentrates
CN108300540A (en) * 2018-03-16 2018-07-20 纳拓润滑技术江苏有限公司 Fire-retardant shield tail sealant of a kind of Biodegradable for shield machine and preparation method thereof
CN108728225A (en) * 2018-07-10 2018-11-02 上海金兆节能科技有限公司 Health environment-friendly lubricating grease and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04337388A (en) * 1991-05-15 1992-11-25 Miyoshi Oil & Fat Co Ltd Metal working oil
CN1219842A (en) * 1996-04-26 1999-06-16 纳幕尔杜邦公司 Soybean oil having high oxidative stability
CN101153236A (en) * 2006-09-29 2008-04-02 中国石油化工股份有限公司 Water-resistant oleosol and method of producing the same
US20110033413A1 (en) * 2007-12-24 2011-02-10 Klaus Kwetkat Method for producing oil-in-water emulsions from self-emulsifying gel concentrates
CN108300540A (en) * 2018-03-16 2018-07-20 纳拓润滑技术江苏有限公司 Fire-retardant shield tail sealant of a kind of Biodegradable for shield machine and preparation method thereof
CN108728225A (en) * 2018-07-10 2018-11-02 上海金兆节能科技有限公司 Health environment-friendly lubricating grease and preparation method thereof

Similar Documents

Publication Publication Date Title
CN109207241B (en) Special shield tail sealing grease for shield tunneling machine and preparation method thereof
CN111004608B (en) Wetting type dust suppressant for road dust emission and preparation method thereof
CN104719116B (en) A kind of artificial soil matrix and its compound method and application
CN104497985B (en) A kind of wet type catches dirt foaming agent
CN101831345A (en) Sealing grease and preparation method and application thereof
CN101787258A (en) Sealing material of shield tail of tunnel shield machine
CN102220111B (en) Leak stopping and wall protecting agent for petroleum drilling fluid and preparation method thereof
CN107400548A (en) A kind of degradable tunneling shield development machine tail seal grease of shield and preparation method thereof
CN105062423A (en) Mine field dust emission inhibitor and preparation method thereof
CN107164029A (en) A kind of environmentally friendly shield machine shield tail seal grease and preparation method thereof
CN101812360A (en) Environmentally-friendly shield tail sealing grease composition for shield development machine
CN103289647B (en) Compound chemical dust suppressant as well as preparation method and application thereof
CN105176635A (en) Novel tunnel shield machine main bearing sealing material
CN103305189B (en) Special dust-depressor for metal mineral powder and ores
CN114369493A (en) Preparation method of biodegradable water-resistant shield tail sealing grease
CN106479441A (en) A kind of microparticle sedimentation agent and its production technology
CN114369486A (en) Biodegradable water-resistant shield tail sealing grease
CN105778867B (en) A kind of solidifying type wet type control dirt wetting agent of anatonosis rush
CN108531151A (en) Push-bench anti-drag mud and preparation method thereof in one planting sand soil property
CN110628386A (en) Composite moisturizing dust suppressant and preparation method thereof
CN110295030A (en) A kind of oil base drilling fluid sealing agent and preparation method thereof
CN108300540A (en) Fire-retardant shield tail sealant of a kind of Biodegradable for shield machine and preparation method thereof
CN206346747U (en) A kind of small diameter central axle drives triumphant formula TBM
CN109076949B (en) Ecological restoration method for karst rock-desertification site in southwest mountain land
CN112409989B (en) Spherical lysine bacillus based tailing surface layer consolidation material and application

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20220419